CN113668048A - Low-resistivity heavily-doped phosphorus silicon single crystal production device and method - Google Patents
Low-resistivity heavily-doped phosphorus silicon single crystal production device and method Download PDFInfo
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- CN113668048A CN113668048A CN202110958466.2A CN202110958466A CN113668048A CN 113668048 A CN113668048 A CN 113668048A CN 202110958466 A CN202110958466 A CN 202110958466A CN 113668048 A CN113668048 A CN 113668048A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/02—Single-crystal growth by pulling from a melt, e.g. Czochralski method adding crystallising materials or reactants forming it in situ to the melt
- C30B15/04—Single-crystal growth by pulling from a melt, e.g. Czochralski method adding crystallising materials or reactants forming it in situ to the melt adding doping materials, e.g. for n-p-junction
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/06—Silicon
Abstract
The invention provides a device and a method for producing low-resistivity heavily phosphorus-doped silicon single crystals, belonging to the technical field of silicon single crystal production. The production device comprises a doping boat made of quartz materials, wherein the doping boat comprises a red phosphorus sublimation chamber and a germanium melting chamber so as to dope phosphorus and germanium into silicon melt at the same time; the top of the red phosphorus sublimation chamber is provided with a plurality of red phosphorus volatilization holes, and the bottom of the germanium melting chamber is provided with a plurality of germanium leakage micropores. And when the red phosphorus is doped, doping simple substance germanium into the silicon melt, wherein the doping amount of the germanium is 1/14-3/14 of the doping amount of the red phosphorus. Practice shows that after the germanium is doped, the performance of the heavily phosphorus-doped silicon single crystal is not influenced, the whole rod rate of the low-resistivity heavily phosphorus-doped silicon single crystal can be effectively improved, the product percent of pass is improved, and waste is reduced. Particularly, when the heavily phosphorus-doped silicon single crystal with the resistivity of less than 0.001 omega-cm is produced, the whole rod rate is improved to 25 percent from less than 10 percent.
Description
Technical Field
The invention belongs to the technical field of silicon single crystal production, and particularly relates to a low-resistivity heavily phosphorus-doped silicon single crystal production device and method.
Background
Phosphorus is a dopant mainly selected by heavily doped N-type silicon single crystals, and has the characteristics of high volatility, flammability, explosiveness, high segregation coefficient and the like. Usually, after the silicon material is melted, phosphorus doping is performed by gas phase doping.
However, with the continuous development of technology, an extremely low resistivity of 0.0015 Ω · cm or less, and even 0.001 Ω · cm or less, of an N-type silicon single crystal is required. Practice shows that the resistivity of the phosphorus-doped silicon single crystal is reduced along with the increase of the phosphorus doping amount, but simultaneously, the rod shaping rate (the probability of forming a complete crystal rod by single drawing) of the phosphorus-doped silicon single crystal is continuously reduced along with the increase of the phosphorus doping amount, and particularly, when the heavily-doped silicon single crystal with the resistivity of less than 0.001 omega-cm is produced, the rod shaping rate is less than 10 percent.
Disclosure of Invention
In view of the above, the invention provides a production device and a production method for a low-resistivity heavily phosphorus-doped silicon single crystal, so as to solve the technical problem that the rod shaping rate is low in the production process of the low-resistivity heavily phosphorus-doped silicon single crystal in the prior art.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a low-resistivity heavily phosphorus-doped silicon single crystal production device comprises a doping boat made of quartz materials, wherein the doping boat comprises a red phosphorus sublimation chamber and a germanium melting chamber so as to dope phosphorus and germanium into silicon melt at the same time; the top of the red phosphorus sublimation chamber is provided with a plurality of red phosphorus volatilization holes, and the bottom of the germanium melting chamber is provided with a plurality of germanium leakage micropores.
Preferably, the pore diameter of the germanium leakage micropores is less than or equal to 1 mm.
Preferably, the germanium melting chamber is arranged below the red phosphorus sublimation chamber and is isolated by a partition plate.
Preferably, the bottom of the germanium melting chamber is provided with a germanium melt diversion slope.
Preferably, the upper end of the red phosphorus sublimation chamber is provided with a hook used for being hung on a seed crystal heavy hammer of the single crystal furnace.
A low-resistivity heavily phosphorus-doped silicon single crystal production method is characterized in that elemental germanium is doped into silicon melt, wherein the doping amount of the elemental germanium is 1/14-3/14 of red phosphorus.
Preferably, the production method of the low-resistivity heavily phosphorus-doped silicon single crystal applies the production device of the low-resistivity heavily phosphorus-doped silicon single crystal, wherein red phosphorus is placed in the red phosphorus sublimation chamber, and is doped into silicon melt after being gasified; elemental germanium is placed in the germanium melting chamber, and flows into the silicon melt from the germanium leakage micropores after melting.
Preferably, the production method of the low-resistivity heavily phosphorus-doped silicon single crystal is used for drawing 8 inches heavily phosphorus-doped silicon single crystal rods by adopting a 24 inches thermal field, wherein the silicon feeding amount is 240kg, the red phosphorus feeding amount is 700 g-1000 g, and the elemental germanium feeding amount is 50 g-150 g.
According to the technical scheme, the invention provides a device and a method for producing low-resistivity heavily phosphorus-doped silicon single crystals, and the device and the method have the beneficial effects that: and when the red phosphorus is doped, doping simple substance germanium into the silicon melt, wherein the doping amount of the germanium is 1/14-3/14 of the doping amount of the red phosphorus. Practice shows that after the germanium is doped, the performance of the heavily phosphorus-doped silicon single crystal is not influenced, the whole rod rate of the low-resistivity heavily phosphorus-doped silicon single crystal can be effectively improved, the product percent of pass is improved, and waste is reduced. Particularly, when the heavily phosphorus-doped silicon single crystal with the resistivity of less than 0.001 omega-cm is produced, the whole rod rate is improved to 25 percent from less than 10 percent.
Drawings
FIG. 1 is a schematic structural diagram of a low resistivity heavily phosphorus-doped silicon single crystal production apparatus.
In the figure: the doping boat 10, the red phosphorus sublimation chamber 100, the red phosphorus volatilization hole 110, the hook 120, the germanium melting chamber 200, the germanium leakage micropore 210, the germanium melt diversion slope 220 and the partition plate 300.
Detailed Description
The technical solutions and effects of the embodiments of the present invention will be further described in detail below with reference to the accompanying drawings of the present invention.
Referring to fig. 1, in one embodiment, an apparatus for producing a low resistivity heavily phosphorus-doped silicon single crystal includes a doping boat 10 made of quartz, the doping boat 10 including a red phosphorus sublimation chamber 100 and a germanium melting chamber 200 for simultaneously doping phosphorus and germanium into a silicon melt. The top of the red phosphorus sublimation chamber 100 is provided with a plurality of red phosphorus volatilization holes 110, and the bottom of the germanium melting chamber 200 is provided with a plurality of germanium leakage micropores 210.
In the embodiment, the Czochralski method is adopted to produce the heavily phosphorus-doped silicon single crystal with the resistivity less than or equal to 0.0015 omega-cm, and the main body of the equipment comprises a single crystal furnace. When the heavily phosphorus-doped silicon single crystal is produced, firstly, the silicon material filled in the crucible is melted, then the doping boat 10 is hung on the seed crystal heavy hammer, the red phosphorus sublimation chamber 100 is used for placing a predetermined amount of red phosphorus (the purity is more than or equal to 99.999%), and the germanium melting chamber 200 is used for placing a predetermined amount of simple substance germanium (the purity is more than or equal to 99.999%). At high temperature, the red phosphorus placed in the red phosphorus sublimation chamber 100 is gasified, diffused by the red phosphorus volatilization hole, and doped in the silicon melt under the action of argon gas flow. After being melted, the elemental germanium placed in the germanium melting chamber 200 is infiltrated through the germanium infiltration micropores 210 and doped in the silicon melt.
Practice shows that when the heavily phosphorus-doped silicon single crystal is produced, particularly the heavily phosphorus-doped silicon single crystal with low resistivity (the resistivity is less than or equal to 0.0015 omega-cm, even the resistivity is less than or equal to 0.001 omega-cm), the elemental germanium is doped into the silicon melt in the red phosphorus doping process, so that the performance of the heavily phosphorus-doped silicon single crystal is not influenced, the rod shaping rate of the heavily phosphorus-doped silicon single crystal with low resistivity can be effectively improved, the product qualification rate is improved, and waste is reduced. Particularly, when the heavily phosphorus-doped silicon single crystal with the resistivity of less than 0.001 omega-cm is produced, the whole rod rate is improved to 25 percent from less than 10 percent.
Preferably, the pore diameter of the germanium percolation micropores 210 is less than or equal to 1mm, for example, the pore diameter of the germanium percolation micropores 210 is 0.5 mm. In principle, the pore diameter of the germanium leakage micropores 210 may be adjusted according to the particle size of the germanium simple substance, so that the germanium simple substance cannot directly enter the silicon melt.
Preferably, the germanium melting chamber 200 is disposed below the red phosphorus sublimation chamber 100 and is isolated by a partition plate 300, so that elemental germanium placed in the germanium melting chamber 200 is close to the high-temperature liquid level of the silicon melt, and sufficient melting of the elemental germanium is ensured.
Further, a germanium melt diversion slope 220 is disposed at the bottom of the germanium melting chamber 200, and solid germanium and molten liquid germanium are gathered towards the concentration region of the germanium leakage micropores 210 under the guiding action of the germanium melt diversion slope 220, so that elemental germanium is fully doped in the silicon melt, residues are reduced, and errors are reduced.
Further, the upper end of the red phosphorus sublimation chamber 100 is provided with a hook 120 for hanging on a single crystal furnace seed crystal weight, so as to hang the doping boat 10 on the single crystal furnace seed crystal weight, and facilitate the doping operation.
In another embodiment of the invention, a method for producing a low-resistivity heavily phosphorus-doped silicon single crystal is provided, wherein elemental germanium is doped into silicon melt, and the doping amount of the elemental germanium is 1/14-3/14 of red phosphorus.
In this embodiment, red phosphorus is doped into the silicon melt by gas phase doping, and elemental germanium may be doped by at least two methods.
Firstly, the simple substance germanium is directly added into the silicon melt along with the silicon material, and is doped into the silicon melt along with the silicon material.
Preferably, the production method of the low-resistivity heavily phosphorus-doped silicon single crystal applies the production device of the low-resistivity heavily phosphorus-doped silicon single crystal, wherein red phosphorus is placed in the red phosphorus sublimation chamber 100, and is doped into the silicon melt after being gasified; elemental germanium is placed in the germanium melting chamber 200 and, after melting, flows into the silicon melt through the germanium leak micro-holes 210.
For example, the production method of the low-resistivity heavily phosphorus-doped silicon single crystal is used for drawing 8 inches heavily phosphorus-doped silicon single crystal rods by adopting a 24 inches thermal field, wherein the silicon feeding amount is 240kg, the red phosphorus feeding amount is 700 g-1000 g, and the elemental germanium feeding amount is 50 g-150 g.
Practice proves that in the process of doping red phosphorus, the silicon melt is simultaneously doped with the elemental germanium, so that the performance of the heavily phosphorus-doped silicon single crystal is not influenced, the whole rod rate of the low-resistivity heavily phosphorus-doped silicon single crystal can be effectively improved, the product qualification rate is improved, and waste is reduced. Particularly, when the heavily phosphorus-doped silicon single crystal with the resistivity of less than 0.001 omega-cm is produced, the whole rod rate is improved to 25 percent from less than 10 percent.
Particularly, when the low-resistivity heavily phosphorus-doped silicon single crystal production device provided by the invention is used for doping, compared with the method of directly adding a germanium simple substance into a silicon material for doping, the whole rod rate of the heavy hammer phosphorus silicon single crystal rod is improved by 5-8%, the product qualification rate is improved, the waste is reduced, and the cost is reduced.
The technical scheme and technical effects of the invention are further explained by the specific examples below. It is worth to be noted that the following specific experimental examples all adopt a single crystal furnace with a 24-inch thermal field, and the process provided by the invention is used for producing 8-inch heavily phosphorus-doped silicon single crystals with low resistivity (the resistivity is below 0.0015 omega-cm to 0.001 omega-cm), and the silicon material feeding amount is 120 kg. In the experimental examples of the present invention, the process parameters which are not particularly limited are generally parameters which can be obtained by those skilled in the art.
Comparative example 1
And doping in a gas phase doping mode according to the resistivity target and the red phosphorus doping amount in the table 1, and counting the whole rod rate. It is to be noted that the red phosphorus doping amount in table 1 is a preferred doping amount required for the heavily phosphorus-doped silicon single crystal to achieve the target resistivity.
Table 1 comparison of comparative example a data
| Target resistivity (omega. cm) | Amount of red phosphorus doped (g) | Rate of whole rod |
| 0.0014 | Disposable doping 700 | 70％ |
| 0.0013 | Disposable doping 760 | 50％ |
| 0.0012 | Disposable doping 800 | 40％ |
| 0.0011 | One-time doping 900 | 20％ |
| 0.001 | One-time doping 1000 | 10％ |
Experimental example 1
And doping in a gas phase doping mode according to the resistivity target and the red phosphorus doping amount shown in the table 2, and counting the whole rod rate. Wherein elemental germanium was charged with the silicon material in the doping amounts shown in table 2. The rest is the same as the comparative example one.
TABLE 2 Experimental example-data comparison
| Target resistivity (omega. cm) | Amount of red phosphorus doped (g) | Pure germanium (g) | Rate of whole rod |
| 0.0014 | Disposable doping 700 | 50g | 71％ |
| 0.0013 | Disposable doping 760 | 50g | 52％ |
| 0.0012 | Disposable doping 800 | 50g | 43％ |
| 0.0011 | One-time doping 900 | 50g | 23％ |
| 0.001 | One-time doping 1000 | 50g | 12％ |
Experimental example two
And doping in a gas phase doping mode according to the resistivity target and the red phosphorus doping amount shown in the table 3, and counting the whole rod rate. Wherein elemental germanium was charged with the silicon material in the doping amounts shown in table 3. The rest is the same as the first experimental example.
TABLE 3 comparison of Experimental examples with data
Experimental example III
And doping in a gas phase doping mode according to the resistivity target and the red phosphorus doping amount shown in the table 4, and counting the whole rod rate. Wherein elemental germanium was charged with the silicon material in the doping amounts shown in table 4. The rest is the same as the first experimental example.
TABLE 4 comparison of the three data of the experimental examples
| Target resistivity (omega. cm) | Amount of red phosphorus doped (g) | Pure germanium (g) | Rate of whole rod |
| 0.0014 | 700 | 150g | 75％ |
| 0.0013 | 760 | 150g | 60％ |
| 0.0012 | 800 | 150g | 50％ |
| 0.0011 | 900 | 150g | 30％ |
| 0.001 | 1000 | 150g | 20％ |
Experimental example four
And doping in a gas phase doping mode according to the resistivity target and the red phosphorus doping amount shown in the table 5, and counting the whole rod rate. In which elemental germanium was charged along with the silicon material in the doping amounts shown in table 5. The rest is the same as the first experimental example.
TABLE 5 Experimental example four data alignment
| Target resistivity (omega. cm) | Amount of red phosphorus doped (g) | Pure germanium (g) | Rate of whole rod |
| 0.0014 | 700 | 200g | 67％ |
| 0.0013 | 760 | 200g | 42％ |
| 0.0012 | 800 | 200g | 32％ |
| 0.0011 | 900 | 200g | 12％ |
| 0.001 | 1000 | 200g | 5％ |
As can be seen from the experimental examples I to IV and the comparative example I, when the heavily phosphorus-doped silicon single crystal is produced, the single germanium and the silicon material are filled together to form the chemical material, and a certain amount of the single germanium is doped, so that the rod shaping rate of the low-resistivity heavily phosphorus-doped silicon single crystal is improved. The increase of the whole rod rate increases with the increase of the germanium doping amount, and when the germanium doping amount reaches 200g, the whole rod rate decreases, possibly caused by excessive germanium doping.
Experimental example five
And doping in a gas phase doping mode according to the resistivity target and the red phosphorus doping amount shown in the table 6, and counting the whole rod rate. Wherein, according to the doping amount shown in table 6, the doping device provided by the present invention is adopted to dope elemental germanium at the same time. The rest is the same as the first experimental example.
TABLE 6 alignment of the five data of the experimental examples
| Target resistivity (omega. cm) | Amount of red phosphorus doped (g) | Pure germanium (g) | Rate of whole rod |
| 0.0014 | Disposable doping 700 | 50g | 74％ |
| 0.0013 | Disposable doping 760 | 50g | 58％ |
| 0.0012 | Disposable doping 800 | 50g | 48％ |
| 0.0011 | One-time doping 900 | 50g | 28％ |
| 0.001 | One-time doping 1000 | 50g | 18％ |
Experimental example six
And doping in a gas phase doping mode according to the resistivity target and the red phosphorus doping amount shown in the table 7, and counting the whole rod rate. Wherein, according to the doping amount shown in table 7, the doping device provided by the present invention is adopted to dope elemental germanium at the same time. The rest is the same as the first experimental example.
TABLE 7 alignment of six data of experimental examples
| Target resistivity (omega. cm) | Amount of red phosphorus doped (g) | Pure germanium (g) | Rate of whole rod |
| 0.0014 | Disposable doping 700 | 100g | 75％ |
| 0.0013 | Disposable doping 760 | 100g | 60％ |
| 0.0012 | Disposable doping 800 | 100g | 50％ |
| 0.0011 | One-time doping 900 | 100g | 30％ |
| 0.001 | One-time doping 1000 | 100g | 20％ |
Experimental example seven
And doping in a gas phase doping mode according to the resistivity target and the red phosphorus doping amount shown in the table 8, and counting the whole rod rate. Wherein, according to the doping amount shown in table 8, the doping apparatus provided by the present invention is adopted to dope elemental germanium at the same time. The rest is the same as the first experimental example.
TABLE 8 comparison of seven data in Experimental examples
| Target resistivity (omega. cm) | Amount of red phosphorus doped (g) | Pure germanium (g) | Rate of whole rod |
| 0.0014 | 700 | 150g | 77％ |
| 0.0013 | 760 | 150g | 65％ |
| 0.0012 | 800 | 150g | 55％ |
| 0.0011 | 900 | 150g | 35％ |
| 0.001 | 1000 | 150g | 25％ |
Experimental example eight
And doping in a gas phase doping mode according to the resistivity target and the red phosphorus doping amount in the table 9, and counting the whole rod rate. Wherein, according to the doping amount shown in table 9, the doping apparatus provided by the present invention is adopted to dope elemental germanium at the same time. The rest is the same as the first experimental example.
TABLE 9 alignment of seven data in Experimental examples
| Target resistivity (omega. cm) | Amount of red phosphorus doped (g) | Pure germanium (g) | Rate of whole rod |
| 0.0014 | 700 | 200g | 68％ |
| 0.0013 | 760 | 200g | 45％ |
| 0.0012 | 800 | 200g | 35％ |
| 0.0011 | 900 | 200g | 15％ |
| 0.001 | 1000 | |
10％ |
Comparing the first to fourth experimental examples and the fifth to eighth experimental examples, it can be seen that the doping device and the doping method provided by the invention can further improve the whole rod rate of the low-resistivity heavily phosphorus-doped silicon single crystal by doping the elemental germanium while doping phosphorus, improve the product qualification rate by about 5-8% on the same scale, reduce waste and reduce cost.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention.
Claims (8)
1. A low resistivity heavily phosphorus-doped silicon single crystal production device comprises a doping boat made of quartz materials, and is characterized in that the doping boat comprises a red phosphorus sublimation chamber and a germanium melting chamber so as to dope phosphorus and germanium into silicon melt at the same time; the top of the red phosphorus sublimation chamber is provided with a plurality of red phosphorus volatilization holes, and the bottom of the germanium melting chamber is provided with a plurality of germanium leakage micropores.
2. The apparatus for producing a low resistivity heavily phosphorus-doped silicon single crystal as claimed in claim 1, wherein the germanium percolation micropores have a pore size of 1mm or less.
3. The low resistivity heavily phosphorus-doped silicon single crystal production apparatus of claim 1, wherein the germanium melting chamber is disposed below the red phosphorus sublimation chamber and is separated therefrom by a partition.
4. The apparatus for producing a low resistivity heavily phosphorus-doped silicon single crystal as claimed in claim 3, wherein a germanium melt guiding slope is provided at a bottom of the germanium melting chamber.
5. The production device of the low-resistivity heavily phosphorus-doped silicon single crystal as claimed in claim 3, wherein a hook for hanging on a seed crystal heavy hammer of the single crystal furnace is arranged at the upper end of the red phosphorus sublimation chamber.
6. The production method of the low-resistivity heavily phosphorus-doped silicon single crystal is characterized by doping elemental germanium into silicon melt, wherein the doping amount of the elemental germanium is 1/14-3/14 of red phosphorus.
7. The method for producing the low-resistivity heavily phosphorus-doped silicon single crystal as claimed in claim 6, wherein the apparatus for producing the low-resistivity heavily phosphorus-doped silicon single crystal as claimed in any one of claims 1 to 5 is used, wherein red phosphorus is placed in the red phosphorus sublimation chamber, and is doped into the silicon melt after being gasified; elemental germanium is placed in the germanium melting chamber, and flows into the silicon melt from the germanium leakage micropores after melting.
8. The production method of the low-resistivity heavily phosphorus-doped silicon single crystal as claimed in claim 7, wherein the production method is used for drawing an 8-inch heavily phosphorus-doped silicon single crystal ingot by adopting a 24-inch thermal field, wherein the silicon dosage is 240kg, the red phosphorus dosage is 700 g-1000 g, and the elemental germanium dosage is 50 g-150 g.
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Cited By (1)
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| CN115323489A (en) * | 2022-08-23 | 2022-11-11 | 宁夏中欣晶圆半导体科技有限公司 | Doping method and doping device for heavily doped silicon single crystal |
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| US20100151667A1 (en) * | 2007-05-31 | 2010-06-17 | Sumco Techxiv Corporation | Dopant implanting method and doping apparatus |
| CN106012010A (en) * | 2016-08-15 | 2016-10-12 | 江苏协鑫硅材料科技发展有限公司 | Method and apparatus for secondary addition of doping agent |
| US20170327966A1 (en) * | 2014-12-24 | 2017-11-16 | Sumco Corporation | Method for producing single crystal |
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| CN1414147A (en) * | 2001-10-26 | 2003-04-30 | 北京有色金属研究总院 | Doping method used in vertical pulling silicon single crystal preparation and its installation |
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| US20100151667A1 (en) * | 2007-05-31 | 2010-06-17 | Sumco Techxiv Corporation | Dopant implanting method and doping apparatus |
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